title: Out-and-back 13C-13C scalar transfers in protein resonance assignment by proton-detected solid-state NMR under ultra-fast MAS.
abstract: We present here (1)H-detected triple-resonance H/N/C experiments that incorporate CO-CA and CA-CB out-and-back scalar-transfer blocks optimized for robust resonance assignment in biosolids under ultra-fast magic-angle spinning (MAS). The first experiment, (H)(CO)CA(CO)NH, yields (1)H-detected inter-residue correlations, in which we record the chemical shifts of the CA spins in the first indirect dimension while during the scalar-transfer delays the coherences are present only on the longer-lived CO spins. The second experiment, (H)(CA)CB(CA)NH, correlates the side-chain CB chemical shifts with the NH of the same residue. These high sensitivity experiments are demonstrated on both fully-protonated and 100%-H(N) back-protonated perdeuterated microcrystalline samples of Acinetobacter phage 205 (AP205) capsids at 60 kHz MAS.
authors.affiliation: CNRS/ENS Lyon/UCB Lyon 1, Centre de RMN à Très Hauts Champs, University of Lyon, Villeurbanne, France.
authors.forename: Emeline
authors.initials: E
authors.lastname: Barbet-Massin
authors.forename: Andrew J
authors.initials: AJ
authors.lastname: Pell
authors.forename: Kristaps
authors.initials: K
authors.lastname: Jaudzems
authors.forename: W Trent
authors.initials: WT
authors.lastname: Franks
authors.forename: Joren S
authors.initials: JS
authors.lastname: Retel
authors.forename: Svetlana
authors.initials: S
authors.lastname: Kotelovica
authors.forename: Inara
authors.initials: I
authors.lastname: Akopjana
authors.forename: Kaspars
authors.initials: K
authors.lastname: Tars
authors.forename: Lyndon
authors.initials: L
authors.lastname: Emsley
authors.forename: Hartmut
authors.initials: H
authors.lastname: Oschkinat
authors.forename: Anne
authors.initials: A
authors.lastname: Lesage
authors.forename: Guido
authors.initials: G
authors.lastname: Pintacuda
mesh_terms: D002247:Carbon Isotopes; D019906:Nuclear Magnetic Resonance, Biomolecular; D011522:Protons; D014764:Viral Proteins / Q000737:chemistry*
chemical_list: D002247:Carbon Isotopes; D011522:Protons; D014764:Viral Proteins